CN108311134A - Diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder and preparation method - Google Patents
Diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder and preparation method Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
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- B01D2258/012—Diesel engines and lean burn gasoline engines
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
- B01J2523/40—Constitutive chemical elements of heterogeneous catalysts of Group IV (IVA or IVB) of the Periodic Table
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
- B01J2523/40—Constitutive chemical elements of heterogeneous catalysts of Group IV (IVA or IVB) of the Periodic Table
- B01J2523/47—Titanium
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
- B01J2523/60—Constitutive chemical elements of heterogeneous catalysts of Group VI (VIA or VIB) of the Periodic Table
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/10—Internal combustion engine [ICE] based vehicles
- Y02T10/12—Improving ICE efficiencies
Abstract
The invention discloses a kind of diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder and preparation methods, belong to carrier coating Material Field.The present invention is to solve the defect of existing SCR catalyst, provides a kind of diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder, is made by following methods：Metatitanic acid is beaten and is disperseed, ammonium hydroxide is added and adjusts pH, obtains slurries；B, by metatitanic acid, ammonium hydroxide is added and adjusts pH, then addition tungsten source and silicon source, after heating and thermal insulation, obtain masterbatch；C, slurries and masterbatch are subjected to press filtration after mixing, filter cake is through calcining, crushing to obtain the final product.The present invention is by adjusting raw material quality control, proportioning, and it is equipped with corresponding preparation process, titanium tungsten silicon composite powder is set not only to have higher specific surface area, and there is high-temperature aging resisting, catalytic temperature is wide, the catalyst of preparation has the performances such as nitric efficiency is high, and scasoning check rate, expulsion rate are low, service life is grown, and has broad application prospects.
Description
Technical field
The invention belongs to carrier coating Material Fields, and in particular to diesel vehicle/steamer tail gas SCR denitration is compound with titanium tungsten silicon
Powder and preparation method.
Background technology
In today that modern industry is more and more flourishing, people more need an environment with fresh air, and PM2.5 is shadow
An important factor for ringing quality of air environment, the large-sized boiler of coal-burning power plant/combusting heavy oil, the exhaust emissions etc. of diesel vehicle/steamer,
All it is the source to form PM2.5；And with the increase of the development of Domestic Automotive Industry and car ownership, the processing of vehicle exhaust
Technology also increasingly causes the concern of people；Nitrogen oxides (NO in diesel vehicle/steamer tail gasx) be administer in main component,
Selective catalytic reduction (SCR) denitration technology is not only widely used in the de- of coal-burning power plant because of its efficient, reliable denitration performance
Nitre system is similarly applied in the denitration technology of the diesel engine vent gas such as diesel vehicle/steamer.
SCR (selective catalytic reduction) gas denitrifying technology refers under the effect of the catalyst, passing through the reduction such as ammonia, urea
Harmful nitrous oxides selectivity in flue gas is catalysed and reduced into clean harmless nitrogen and water, realizes qualified discharge, denitration by agent
Catalyst is the key that implement this technology and core.Typical commercial SCR catalyst is with TiO2For carrier, with V2O5-WO3
(MoO3) etc. metal oxide containing precious metals be active component.Currently, vehicle/SCR catalyst peculiar to vessel selects the metal and ceramic honey comb to be mostly
Carrier is prepared using titanium tungsten vanadium or titanium tungsten molybdenum vanadium metal oxide as coating material and active material.But due to vehicle/peculiar to vessel
SCR catalyst needs to meet the particular/special requirements such as ageing-resistant and high intensity, low-sulfur, the high-specific surface area under high temperature, current big multiselect
It is the carrier and coating material of full import, application cost is higher；Therefore, research is suitable for diesel vehicle/steamer vent gas treatment
Efficient, heat resistant and high intensity SCR denitration carrier and its coating material and to realize that production domesticization has very big
Realistic meaning and economic value.
Chinese patent CN101757907 discloses a kind of system of honeycomb-shaped SCR denitrating catalyst tungstenic titanium dioxide powder
Standby technology, group are divided into TiO2-WO3Powder, but it is only applicable to coal-fired plant flue gas denitration, and it includes bavin to be not appropriate for moving source
The tail gas denitration of oily vehicle/steamer；Patent CN103769080 discloses a kind of diesel car tail gas refining SCR catalyst and carrier applies
The preparation method of layer material, including TiO2-WO3The technology of preparing of powder, technology of preparing and common SCR catalyst carrier
TiO2-WO3As the preparation of powder, powder cannot solve the problems, such as catalyst high-temperature aging resisting without specially treated；Patent
CN103908970 discloses a kind of monoblock type SCR honeycomb catalysts and preparation method thereof for exhaust gas from diesel vehicle processing, introduces
A kind of technology of preparing of SCR catalyst carrier coating material, group are divided into ZrO2-TiO2Composite oxides, method is using precipitation
Prepared by method, help active material WO3All use rear addition method, cost of manufacture higher with active material vanadium.
Invention content
Technical problem to be solved by the invention is to provide a kind of SCR catalysts as diesel vehicle/steamer vent gas treatment
Carrier nanoscale TiO2-WO3-SiO2Composite powder not only has high specific surface area, chemical mobility of the surface height and meets diesel vehicle
With the heat resistant of catalyst, processing performance is good the advantages that, and it is excellent with higher mechanical strength and resistance to erosion intensity
Point, and it is of low cost, preparation process is simple, the denitrating catalyst being prepared by the product has intensity big, service life is long,
The advantages that high catalytic efficiency.
There is provided a kind of diesel vehicle/steamer tail gas SCR for technological means used by the present invention solves above-mentioned technical problem
Denitration titanium tungsten silicon composite powder, is prepared by following methods：
A, it is 22%~25% metatitanic acid mashing to be dispersed to the mass fraction in terms of titanium dioxide, and ammonium hydroxide is added and adjusts
PH is stirred evenly, and obtains slurries, spare；
B, it is 15%~20% by mass fraction of the metatitanic acid mashing dispersion in terms of titanium dioxide, ammonium hydroxide is added and adjusts pH,
Then it is added tungsten source and silicon source, after heating and thermal insulation, obtains masterbatch；
C, masterbatch obtained by slurries obtained by step a and step b is subjected to press filtration after mixing, after gained filtration cakes torrefaction, into
Row calcining, calcining resulting material obtain diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder through crushing.
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is in titanium tungsten silicon composite powder, in step a, it is described partially
The mass concentration of metatitanic acid is 25%~30%, metatitanic acid iron content≤100ppm, and particle diameter distribution D50 is 0.8~1.0 μm.
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is in titanium tungsten silicon composite powder, in step b, it is described partially
The mass concentration of metatitanic acid is 25%~30%, metatitanic acid iron content≤100ppm, and particle diameter distribution D50 is 0.8~1.0 μm.
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is in titanium tungsten silicon composite powder, inclined titanium described in step a
Mass ratio of the dosage of metatitanic acid in terms of titanium dioxide described in the dosage and step b of acid is 0.5~1.5：1.
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is in titanium tungsten silicon composite powder, in step a, the ammonia
The addition of water is regulation system pH to 7.5~8.8.
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is in titanium tungsten silicon composite powder, in step b, the ammonia
The addition of water is regulation system pH to 7.5~8.8.
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is in titanium tungsten silicon composite powder, in step b, the tungsten
Source is para-tungstic acid amine, WO3Mass content is 88~90%.
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is in titanium tungsten silicon composite powder, in step b, the tungsten
The addition in source WO in masterbatch in order to control3Mass content is 6%~20%.
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is in titanium tungsten silicon composite powder, in step b, the silicon
Source is Ludox；The SiO of the Ludox2Mass content is 25%~35%, and grain size is 10~20nm, and specific surface area is not less than
600m2/g。
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is in titanium tungsten silicon composite powder, in step b, the silicon
The dosage in source SiO in masterbatch in order to control2Mass content is 3%~7%.
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is in titanium tungsten silicon composite powder, in step b, it is described plus
The temperature of heat heat preservation is 70 DEG C~80 DEG C, and the time is 1h~3h.
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is in titanium tungsten silicon composite powder, in step b, it is described plus
During heat heat preservation, it is 7.5~8.8 that addition ammonium hydroxide, which keeps system pH,.
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is in titanium tungsten silicon composite powder, in step a, the ammonia
A concentration of the 18%~21% of water.
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is in titanium tungsten silicon composite powder, in step b, the ammonia
A concentration of the 18%~21% of water.
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is in titanium tungsten silicon composite powder, described dry in step c
Dry temperature is 250 DEG C~300 DEG C, and drying time is 1.5~2.5h.
Wherein, diesel vehicle described above/steamer tail gas SCR denitration is described to forge in step c in titanium tungsten silicon composite powder
Burn be segmented calcine, i.e., at 350 DEG C~380 DEG C calcine 60~120min, 480 DEG C~500 DEG C calcining 40~80min, 580 DEG C
~620 DEG C of 40~80min of calcining.
Diesel vehicle provided by the invention/steamer tail gas SCR denitration can be prepared into titanium tungsten silicon composite powder by the above method
It arrives comprising following components in percentage by weight：Titanium dioxide 84%~93%, tungstic acid 3%~10%, silica
1.5%~3.5%, sulfate radical 0.5%~3.0%, water 0.5%~2.0%.
The granularity of diesel vehicle provided by the invention/steamer tail gas SCR denitration titanium tungsten silicon composite powder is -325 mesh.
Beneficial effects of the present invention：
Metatitanic acid of the present invention is bigger serface metatitanic acid, provides multistage and cyclone classification technology is used in conjunction, make
Product metatitanic acid particle size uniformly (D50 is controlled at 0.8~1.0 μm) is obtained, distribution is concentrated, large specific surface area, and binding performance is excellent
It is different；The SiO of Ludox of the present invention2Mass content is 25%~35%, and grain size is 10~20nm, Ludox and routine
Silicon source white carbon compares specific surface area >=600m with bigger2/ g, stronger adsorptivity and higher dispersibility, use Ludox
TiO as silicon source production2-WO3-SiO2Composite powder denitration efficiency higher, more preferably, service life is more for anti-aging, high temperature resistant property
It is long；Simultaneously because silicon dioxide molecules bond energy is big in Ludox, it can be before ensureing mechanical strength and other denitration performances
It puts and reduces noble metal WO3Dosage；The curing step for providing heating and thermal insulation, can further promote titanium dioxide and silica
And the combination of tungstic acid, it is allowed to that combination is more secured, the product absorption of production, binding ability are stronger, and expulsion rate is low, denitration efficiency
Higher, anti-aging property is more preferable, prolongs the service life；The dosage of Ludox can be reduced simultaneously so that product is in SiO2Content drops
It remains to reach higher denitration efficiency in the case of low, achieve the purpose that the consumption for reducing noble metal and reduces production cost.
The present invention provides a kind of diesel oil by adjusting to raw material quality control, proportioning, and being equipped with corresponding preparation process
Vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder not only has higher specific surface area, but also has high-temperature aging resisting, urges
Change the performances such as temperature is wide, and the catalyst of preparation is high with nitric efficiency, and scasoning check rate, expulsion rate are low, service life is grown, has
Wide application prospect.
Specific implementation mode
Specifically, a kind of diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder, is prepared by following methods：
A, it is 22%~25% metatitanic acid mashing to be dispersed to the mass fraction in terms of titanium dioxide, and ammonium hydroxide is added and adjusts
PH is stirred evenly, and obtains slurries, spare；
B, it is 18%~20% by mass fraction of the metatitanic acid mashing dispersion in terms of titanium dioxide, ammonium hydroxide is added and adjusts pH,
Then it is added tungsten source and silicon source, after heating and thermal insulation, obtains masterbatch；
C, masterbatch obtained by slurries obtained by step a and step b is subjected to press filtration after mixing, after gained filtration cakes torrefaction, into
Row calcining, calcining resulting material obtain diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder through crushing.
Raw material metatitanic acid mass concentration is 25%~30% in the present invention, metatitanic acid iron content≤100ppm, grain size point
Cloth D50 is 0.8~1.0 μm, can be used but is not limited to following methods and is prepared：
A, titanium slag and titanium ore are subjected to acidolysis respectively, the mass ratio of titanium slag and titanium ore is 1.5~2.5：1, titanium slag is used
96.5%~98.3% sulfuric acid carries out acidolysis, and it is 1.65~1.75 that acid, which is measured with the mass ratio of titanium slag,：1, titanium ore with 91.5%~
93% sulfuric acid carries out acidolysis, and it is 1.45~1.55 that acid, which is measured with the mass ratio of titanium ore,：1；Titanium slag acidolysis terminates post curing 3h~5h, titanium
Mine acidolysis terminates post curing 2h~3h；Curing is completed plus water extraction, merges the two leaching liquid, obtains titanium liquid；In the titanium liquid：It is dense
Degree is with TiO2It is calculated as 150 ± 5g/L, Ti3+For 1.5 ± 0.5g/L, F values are 1.8 ± 0.25, and iron titanium ratio is 0.3 ± 0.05, is stablized
Property >=600mL；
B, titanium liquid obtained by step a is filtered at 15~55 DEG C, obtains clear titanium liquid (solid content≤0.03%), clear titanium liquid carries out dense
Contracting, the concentration of titanium liquid is with TiO after control concentration2It is calculated as 200 ± 5g/L；
C, the titanium liquid after being concentrated in step b is mixed with crystal seed, is hydrolyzed, reaction system is stirred in 94~96 DEG C of constant temperature
20~40min of curing is mixed, being heated after curing makes reaction system reach boiling, (general after reaction system becomes steel grey
Need 10~15min), constant temperature stands 20~40min；Reaction system, which is heated, again and is stirred makes it reach boiling again；Boiling
After make reaction system that 170~190min of slight boiling condition, hydrolysis be kept to terminate at 30~100mmHg, obtain hydrolysis metatitanic acid；It is described
Crystal seed is prepared by following methods：Crystal seed titanium liquid and sodium hydroxide solution be warming up to 88~92 DEG C between when, by crystal seed titanium liquid
It is added in two portions in sodium hydroxide solution, the 1/3 of crystal seed titanium liquid total volume is added for the first time, has been added in 60~90 seconds
Finish；The 2/3 of second of addition crystal seed titanium liquid total volume, is added in 30~50 seconds and finishes；It is added and finishes second for the first time
The time being initially added into is separated by 15~25 seconds, forms mixed liquor；Mixed liquor is warming up to 95~97 DEG C, stability is surveyed in heat preservation, when
When stability reaches 100~125mL, crystal seed is obtained；The concentration of the crystal seed titanium liquid is with TiO2It is calculated as 200 ± 5g/L；The hydrogen-oxygen
The mass concentration for changing sodium solution is 8 ± 0.2%；The addition of the sodium hydroxide solution is calculated as TiO in crystal seed titanium liquid with NaOH2
The 20%~25% of quality；The concentration of the crystal seed is with TiO2It is calculated as 148 ± 2.5g/L；The norm controlling of the hydrolysis metatitanic acid
For：Concentration is with TiO2It is calculated as 165 ± 5g/L, Ti3+For 1.5 ± 0.5g/L, percent hydrolysis 95.5 ± 0.5%, pumping speed 150 ± 50 ", it sinks
150 ± 25mm of drop height；
D, hydrolysis metatitanic acid obtained by step c is washed in leaf filter, control upper piece thickness 40~50mm, 0.05MPa
≤ vacuum degree (preferably 0.05MPa≤vacuum degree≤0.1MPa), 2~4h of washing time；Water is added to size mixing the metatitanic acid after washing
To slurry Ti content with TiO2It is calculated as 260~300g/L, adds Ti3+And sulfuric acid, slurry index after control bleaching：Ti3+Content
For 0.5~2g/L, free acid (i.e. H+) it is 25~60g/L；Then slurry after bleaching is rinsed in leaf filter, it is desirable that on
Piece 30~40mm of thickness, 0.05MPa≤vacuum degree (preferably 0.05MPa≤vacuum degree≤0.1MPa), 3~5h of rinsing time is obtained
The metatitanic acid qualified to rinsing, metatitanic acid iron content≤100ppm；
F, cyclone classification technology is used in conjunction using multistage in the qualified metatitanic acid of rinsing obtained by step d and is classified (slurry
Carried out under state), control slurry D50 is 0.8~1.0 μm, you can obtains can be used as in the raw material metatitanic acid of the present invention.
Metatitanic acid of the present invention is that (specific surface area is 300 ± 50m to bigger serface metatitanic acid2/ g), in conjunction with water
Increase multistage after washing and cyclone classification technology is used in conjunction so that uniformly (D50 is controlled in 0.8~1.0 μ product metatitanic acid particle size
M), distribution is concentrated, large specific surface area, and binding performance is excellent.
Experiment find, since tungstic acid, dioxide-containing silica are relatively low in titanium tungsten silicon composite powder of the present invention, need with
Combination titanium dioxide it is less, by the dosage of metatitanic acid described in the dosage of metatitanic acid described in step a of the present invention and step b
Control is 0.5~1.5 in the mass ratio in terms of titanium dioxide：1, it can not only ensure further by heating curing in step b
The combination for promoting titanium dioxide and silica and tungstic acid, it is more secured to be allowed to combination so that product is in SiO2Content reduces
In the case of remain to reach higher denitration efficiency, achieve the purpose that reduce noble metal consumption and reduce production cost, simultaneously
Energy consumption is saved, is further reduced the cost.Same batch can be used in metatitanic acid used in step a and step b of the present invention, can also be used
Different batches, as long as meeting quality requirement and the dosage requirement of the present invention.
In step a, the mass fraction after control metatitanic acid mashing dispersion in terms of titanium dioxide is 22%~25%, is then added
Enter ammonia water conditioning system pH to 7.5~8.8；In step b, the mass fraction after control metatitanic acid mashing dispersion in terms of titanium dioxide
It is 18%~20%, ammonia water conditioning system pH is then added to 7.5~8.8, and during heating and thermal insulation, adds ammonium hydroxide
Holding system pH is 7.5~8.8.
The purpose that concentration of slurry is controlled in step a and step b is on the one hand to make TiO2、WO3、SiO2Three is fully mixed
It closes, uniformly combines, be on the other hand to make the SO in metatitanic acid slurries4 2-It is combined into (NH with ammonium hydroxide4)2SO4, convenient follow-up
Calcination process removes, and removes SO4 2-The reason of be on the one hand to prevent S constituent contents are excessively high from causing catalyst poisoning, on the other hand again must
It must keep the SO of appropriate concentration4 2-(0.5%~3.0%) makes SO in product4 2-By with TiO2Surface coordination, with TiO2Between shape
At chelate bonds, is conducive to the mesoporous holding of material and mesoporous distribution is more reasonable, to make composite granule that there is very high Kong Rong
And specific surface area, to ensure that high catalytic activity；Further, since step b needs to carry out heating and thermal insulation processing, it is therefore desirable to point
The beating consistency of metatitanic acid in other rate-determining steps a and step b, if step a concentration of slurry is consistent with step b concentration of slurry,
It after calcination processing, will lead in titanium tungsten silicon composite powder product system that sulfate radical content is relatively low, influence its performance.Institute in the present invention
Using a concentration of the 18%~21% of ammonium hydroxide.
In the present invention, para-tungstic acid amine, WO can be used in tungsten source3Mass content is 88~90%, and the addition in tungsten source is control
WO in masterbatch processed3Mass content is 6%~20%；Ludox, the SiO of Ludox can be used in silicon source2Mass content be 25%~
35%, grain size is 10~20nm, Ludox specific surface area >=600m with bigger compared with conventional silicon source white carbon2/ g, more
Strong adsorptivity and higher dispersibility, the TiO for using Ludox to be produced as silicon source2-WO3-SiO2Composite powder denitration efficiency is more
Height, more preferably, the service life is longer for anti-aging, high temperature resistant property；It, can be simultaneously because silicon dioxide molecules bond energy is big in Ludox
Ensure to reduce noble metal WO under the premise of mechanical strength and other denitration performances3Dosage；The dosage of the silicon source is control
SiO in masterbatch processed2Mass content is 3%~7%.
In step b of the present invention, after tungsten source and silicon source is added, increase the curing step of heating and thermal insulation, by 70 DEG C~
80 DEG C of curing 1h~3h, can further promote the combination of titanium dioxide and silica and tungstic acid, and it is more secured to be allowed to combination,
The product absorption of production, binding ability are stronger, and expulsion rate is low, and denitration efficiency higher, anti-aging property is more preferable, extend and use the longevity
Life；The dosage of Ludox can be reduced simultaneously so that product is in SiO2Content remains to reach higher denitration effect in the case of reducing
Rate achievees the purpose that the consumption for reducing noble metal and reduces production cost.
In step c, masterbatch obtained by slurries obtained by step a and step b is subjected to press filtration, gained filter cake 250 after mixing
DEG C~300 DEG C of dry 1.5~2.5h after, calcined, calcining using segmented calcine, i.e., at 350 DEG C~380 DEG C calcining 60~
120min, 480 DEG C~500 DEG C calcinings 40~80min, 580 DEG C~620 DEG C 40~80min of calcining calcine resulting material crushing
Afterwards, it can all be sieved by 325 mesh, obtain diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder.
Diesel vehicle provided by the invention/steamer tail gas SCR denitration can be prepared into titanium tungsten silicon composite powder by the above method
It arrives comprising following components in percentage by weight：Titanium dioxide 84%~93%, tungstic acid 3%~10%, silica
1.5%~3.5%, sulfate radical 0.5%~3.0%, water 0.5%~2.0%.
Below by test example and embodiment, invention is further described in detail, but does not therefore protect the present invention
Scope limitation is among the embodiment described range.
In the embodiment of the present invention, the mass concentration of used metatitanic acid is 25%~30%, metatitanic acid iron content≤
100ppm, particle diameter distribution D50 are 0.8~1.0 μm, and specific surface area is 300 ± 50m2/g；WO in ammonium paratungstate3Mass content is
88%~90%；SiO in Ludox2Mass content 25%~35%, grain size 10nm~20nm, specific surface area >=600m2/g；Ammonia
Water concentration is 18%~21%.
Embodiment 1
A, 10Kg metatitanic acids are weighed (by TiO2Meter), two parts are divided into, portion is added in the reactor with agitating device,
Deionized water is added, it is 23% that mashing, which is dispersed to the mass fraction in terms of titanium dioxide, and ammonium hydroxide is added and adjusts pH to 7.93, stirring
Uniformly, slurries are obtained, it is spare；
B, another is added in the reactor with agitating device, and deionized water is added, and mashing is dispersed to titanium dioxide
The mass fraction of meter is 20%, and ammonium hydroxide is added and adjusts pH to 7.91, ammonium paratungstate (APT) 1.1kg, Ludox are added into slurry
1.1kg is heated to 75 DEG C and keeps the temperature 2h, and during heating and thermal insulation, it is 7.5~8.8 that addition ammonium hydroxide, which keeps system pH, is obtained female
Material；
C, slurries and masterbatch are mixed evenly, press filtration obtains blocky filter cake, and filter cake enters after 250 DEG C of dry 2h
Rotary kiln is calcined, and 1.5h is calcined at 350 DEG C~380 DEG C, 480 DEG C~500 DEG C calcining 1h, 580 DEG C~620 DEG C are calcined 1h, will be calcined
Obtained calcining falls the shearing rotor grinding of kiln material and crushes (after crushing 325 mesh full by), is prepared into powdered titanium dioxide-
Tungstic acid-silica composite powder (i.e. diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder).
Embodiment 2
A, 10Kg metatitanic acids are weighed (by TiO2Meter), two parts are divided into, portion is added in the reactor with agitating device,
Deionized water is added, it is 23% that mashing, which is dispersed to the mass fraction in terms of titanium dioxide, and ammonium hydroxide is added and adjusts pH to 7.76, stirring
Uniformly, slurries are obtained, it is spare；
B, another is added in the reactor with agitating device, and deionized water is added, and mashing is dispersed to titanium dioxide
The mass fraction of meter is 18%, and ammonium hydroxide is added and adjusts pH to 7.84, ammonium paratungstate (APT) 1.1kg, Ludox are added into slurry
0.52kg is heated to 75 DEG C and keeps the temperature 2h, and during heating and thermal insulation, it is 7.5~8.8 that addition ammonium hydroxide, which keeps system pH, is obtained female
Material；
C, slurries and masterbatch are mixed evenly, press filtration obtains blocky filter cake, and filter cake enters after 250 DEG C of dry 2h
Rotary kiln is calcined, and 1.5h is calcined at 350 DEG C~380 DEG C, 480 DEG C~500 DEG C calcining 1h, 580 DEG C~620 DEG C are calcined 1h, will be calcined
Obtained calcining falls the shearing rotor grinding of kiln material and crushes (after crushing 325 mesh full by), is prepared into powdered titanium dioxide-
Tungstic acid-silica composite powder.
Embodiment 3
A, 10Kg metatitanic acids are weighed (by TiO2Meter), two parts are divided into, portion is added in the reactor with agitating device,
Deionized water is added, it is 23% that mashing, which is dispersed to the mass fraction in terms of titanium dioxide, and ammonium hydroxide is added and adjusts pH to 8.53, stirring
Uniformly, slurries are obtained, it is spare；
B, another is added in the reactor with agitating device, and deionized water is added, and mashing is dispersed to titanium dioxide
The mass fraction of meter is 18%, and ammonium hydroxide is added and adjusts pH to 8.49, ammonium paratungstate (APT) 0.4kg, Ludox are added into slurry
1.1kg is heated to 75 DEG C and keeps the temperature 2h, and during heating and thermal insulation, it is 7.5~8.8 that addition ammonium hydroxide, which keeps system pH, is obtained female
Material；
C, slurries and masterbatch are mixed evenly, press filtration obtains blocky filter cake, and filter cake enters after 250 DEG C of dry 2h
Rotary kiln is calcined, and 1.5h is calcined at 350 DEG C~380 DEG C, 480 DEG C~500 DEG C calcining 1h, 600 DEG C~630 DEG C are calcined 1h, will be calcined
Obtained calcining falls the shearing rotor grinding of kiln material and crushes (after crushing 325 mesh full by), is prepared into powdered titanium dioxide-
Tungstic acid-silica composite powder.
Embodiment 4
A, 10Kg metatitanic acids are weighed (by TiO2Meter), two parts are divided into, portion is added in the reactor with agitating device,
Deionized water is added, it is 23% that mashing, which is dispersed to the mass fraction in terms of titanium dioxide, and ammonium hydroxide is added and adjusts pH to 8.36, stirring
Uniformly, slurries are obtained, it is spare；
B, another is added in the reactor with agitating device, and deionized water is added, and mashing is dispersed to titanium dioxide
The mass fraction of meter is 18%, and ammonium hydroxide is added and adjusts pH to 8.29, and it is molten that ammonium paratungstate (APT) 0.95kg, silicon are added into slurry
Glue 1kg is heated to 75 DEG C and keeps the temperature 2h, and during heating and thermal insulation, it is 7.5~8.8 that addition ammonium hydroxide, which keeps system pH, is obtained female
Material；
C, slurries and masterbatch are mixed evenly, press filtration obtains blocky filter cake, and filter cake enters after 250 DEG C of dry 2h
Rotary kiln is calcined, and 1.5h is calcined at 350 DEG C~380 DEG C, 480 DEG C~500 DEG C calcining 1h, 580 DEG C~620 DEG C are calcined 1h, will be calcined
Obtained calcining falls the shearing rotor grinding of kiln material and crushes (after crushing 325 mesh full by), is prepared into powdered titanium dioxide-
Tungstic acid-silica composite powder.
Embodiment 5
A, 10Kg metatitanic acids are weighed (by TiO2Meter), two parts are divided into, portion is added in the reactor with agitating device,
Deionized water is added, it is 25% that mashing, which is dispersed to the mass fraction in terms of titanium dioxide, and ammonium hydroxide is added and adjusts pH to 8.31, stirring
Uniformly, slurries are obtained, it is spare；
B, another is added in the reactor with agitating device, and deionized water is added, and mashing is dispersed to titanium dioxide
The mass fraction of meter is 20%, and ammonium hydroxide is added and adjusts pH to 8.37, and it is molten that ammonium paratungstate (APT) 0.65kg, silicon are added into slurry
Glue 1kg is heated to 75 DEG C and keeps the temperature 2h, and during heating and thermal insulation, it is 7.5~8.8 that addition ammonium hydroxide, which keeps system pH, is obtained female
Material；
C, slurries and masterbatch are mixed evenly, press filtration obtains blocky filter cake, and filter cake enters after 250 DEG C of dry 2h
Rotary kiln is calcined, and 1.5h is calcined at 350 DEG C~380 DEG C, 480 DEG C~500 DEG C calcining 1h, 580 DEG C~620 DEG C are calcined 1h, will be calcined
Obtained calcining falls the shearing rotor grinding of kiln material and crushes (after crushing 325 mesh full by), is prepared into powdered titanium dioxide-
Tungstic acid-silica composite powder.
Embodiment 6
A, 10Kg metatitanic acids are weighed (by TiO2Meter), two parts are divided into, portion is added in the reactor with agitating device,
Deionized water is added, it is 25% that mashing, which is dispersed to the mass fraction in terms of titanium dioxide, and ammonium hydroxide is added and adjusts pH to 8.31, stirring
Uniformly, slurries are obtained, it is spare；
B, another is added in the reactor with agitating device, and deionized water is added, and mashing is dispersed to titanium dioxide
The mass fraction of meter is 20%, and ammonium hydroxide is added and adjusts pH to 8.37, ammonium paratungstate (APT) 1.3kg, Ludox are added into slurry
0.52kg is heated to 75 DEG C and keeps the temperature 2h, and during heating and thermal insulation, it is 7.5~8.8 that addition ammonium hydroxide, which keeps system pH, is obtained female
Material；
C, slurries and masterbatch are mixed evenly, press filtration obtains blocky filter cake, and filter cake enters after 250 DEG C of dry 2h
Rotary kiln is calcined, and 1.5h is calcined at 350 DEG C~380 DEG C, 480 DEG C~500 DEG C calcining 1h, 600 DEG C~640 DEG C are calcined 1h, will be calcined
Obtained calcining falls the shearing rotor grinding of kiln material and crushes (after crushing 325 mesh full by), is prepared into powdered titanium dioxide-
Tungstic acid-silica composite powder.
Comparative example 1
Metatitanic acid, tungsten source are same as Example 5, and the 1kg silicon in silicon source selection white carbon 0.35kg alternative embodiments 5 is molten
Titanium dioxide-tungstic acid-silica composite powder is made according to 5 identical production method of embodiment in glue.
Comparative example 2
Metatitanic acid, tungsten source, silicon source are same as Example 5, production method be metatitanic acid by mashing, adjust pH, be added tungsten source,
Silicon source, press filtration, calcining crush obtained titanium dioxide-tungstic acid-silica composite powder, and concrete operations are：
10Kg metatitanic acids are weighed (by TiO2Meter), it is added in the reactor with agitating device, deionized water, mashing is added
It is 20% to be dispersed to the mass fraction in terms of titanium dioxide, and ammonium hydroxide is added, and it is 8.41 to make system pH, and para-tungstic acid is added into slurry
Ammonium (APT) 0.65kg, Ludox 1kg, press filtration obtain blocky filter cake, and filter cake is calcined after 250 DEG C of dry 2h into rotary kiln,
350 DEG C~380 DEG C calcining 1.5h, 480 DEG C~500 DEG C calcining 1h, 580 DEG C~620 DEG C are calcined 1h, will be calcined obtained calcining and be fallen
The shearing rotor grinding of kiln material crushes (after crushing 325 mesh full by), is prepared into powdered titanium dioxide-tungstic acid-two
Silica composite powder.
Compound powder component, property and application performance detection
Examples 1 to 6 and comparative example 1~2 prepare the component of gained titanium dioxide-tungstic acid-silica composite powder
And property test is shown in Table 1, specific data are as follows：
The compound powder component of 1 titanium tungsten silicon of table and performance detection
It is obtained by data in table 1 it is found that the present invention is adjusted using Ludox as silicon source, and to technological parameter
Product has preferable anti-aging property, and present invention energy in the case of silica and relatively low tungstic acid content
Ensure specific surface area, anti-aging area and other performance indicators of product.
Examples 1 to 6 and comparative example 1~2 are prepared into gained titanium dioxide-tungstic acid-silica composite powder through phase
It is smeared with coating processes and carries out application performance detection after catalyst is made, the results are shown in Table 2.
2 application performance of table detects
From the data in table 2, it can be seen that the titanium tungsten silicon composite powder of the present invention has higher denitrification percent, scasoning check rate and expulsion rate
It is relatively low.
Claims (10)
1. diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder, it is characterised in that：It is prepared by following methods：
A, it is 22%~25% metatitanic acid mashing to be dispersed to the mass fraction in terms of titanium dioxide, and ammonium hydroxide is added and adjusts pH, stirs
It mixes uniformly, obtains slurries, it is spare；
B, it is 15%~20% by mass fraction of the metatitanic acid mashing dispersion in terms of titanium dioxide, ammonium hydroxide is added and adjusts pH, then
It is added tungsten source and silicon source, after heating and thermal insulation, obtains masterbatch；
C, masterbatch obtained by slurries obtained by step a and step b is subjected to press filtration after mixing, after gained filtration cakes torrefaction, is forged
It burns, calcining resulting material obtains diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder through crushing.
2. diesel vehicle according to claim 1/steamer tail gas SCR denitration titanium tungsten silicon composite powder, it is characterised in that：Step
In a and step b, the mass concentration of the metatitanic acid is 25%~30%, metatitanic acid iron content≤100ppm, particle diameter distribution D50
It is 0.8~1.0 μm.
3. diesel vehicle according to claim 1 or 2/steamer tail gas SCR denitration titanium tungsten silicon composite powder, it is characterised in that：
Mass ratio of the dosage of metatitanic acid in terms of titanium dioxide described in the dosage of metatitanic acid described in step a and step b is 0.5~
1.5：1.
4. diesel vehicle according to claim 1/steamer tail gas SCR denitration titanium tungsten silicon composite powder, it is characterised in that：Step
In a, the addition of the ammonium hydroxide is regulation system pH to 7.5~8.8；In step b, the addition of the ammonium hydroxide is regulation system
PH to 7.5~8.8.
5. diesel vehicle according to claim 1/steamer tail gas SCR denitration titanium tungsten silicon composite powder, it is characterised in that：Step
In b, the tungsten source is para-tungstic acid amine, WO3Mass content is 88~90%；The addition in tungsten source WO in masterbatch in order to control3
Mass content is 6%~20%.
6. diesel vehicle according to claim 1/steamer tail gas SCR denitration titanium tungsten silicon composite powder, it is characterised in that：Step
In b, the silicon source is Ludox；The SiO of the Ludox2Mass content is 25%~35%, and grain size is 10~20nm, compares table
Area is not less than 600m2/g；The dosage of silicon source SiO in masterbatch in order to control2Mass content is 3%~7%.
7. diesel vehicle according to claim 1/steamer tail gas SCR denitration titanium tungsten silicon composite powder, it is characterised in that：Step
In b, the temperature of the heating and thermal insulation is 70 DEG C~80 DEG C, and the time is 1h~3h；In step b, during the heating and thermal insulation,
It is 7.5~8.8 to add ammonium hydroxide and keep system pH.
8. according to claim 1~7 any one of them diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder, feature
It is：In step a and step b, a concentration of the 18%~21% of the ammonium hydroxide.
9. diesel vehicle according to claim 1/steamer tail gas SCR denitration titanium tungsten silicon composite powder, it is characterised in that：Step
In c, the temperature of the drying is 250~300 DEG C, and drying time is 1.5~2.5h；The calcining is that segmented is calcined, that is, is existed
350 DEG C~380 DEG C calcining 60~120min, 480 DEG C~500 DEG C calcining 40~80min, 580 DEG C~620 DEG C calcining 40~
80min。
10. special according to claim 1~9 any one of them diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder
Sign is：The diesel vehicle/steamer tail gas SCR denitration titanium tungsten silicon composite powder includes following components in percentage by weight：Dioxy
Change titanium 84%~93%, tungstic acid 3%~10%, silica 1 .5%~3.5%, sulfate radical 0.5%~3.0%, water
0.5%~2.0%.
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